SU1293180A1 - Method of producing nъnъ-bis-(2-phthalimidoethul)-piperazine - Google Patents

Abstract

This invention relates to substituted heterocyclic compounds, in particular to the preparation of N, N - -bis- (2-phthalimidoethyl) piperazine (PSF), which is used to synthesize N, N-bis- (2-aminostil) piperazine. Increasing the yield of FIP, simplifying the process and reducing its duration is achieved by using a different source, then the product and carrying out the process under certain conditions. 2.1: 1, and 180- followed by treatment with dibromoethane and potassium carbonate, seizing. - in the molar ratio of 5.8-17.4:: 1-3 per 1 mole of the initial TD, at 100-132 ° C. The yield increased to 45%. 1 tab. rsD (Ui

Description

112931

This invention relates to a process for the preparation of an N, N-bis- (2-phthalimidoethyl) piperazine of formula 1

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 -

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which is used in organic synthesis to obtain N, N -bis- (2-aminoethyl) piperazine.

The purpose of the invention is to increase the yield of the target product, simplify the process and shorten its duration by using 1, A, 7,10-tetraazadecane (triethylene tetraamine), which is introduced to react with phthalimide at 180-, as one of the initial reagents, and processing the resulting reaction mixture dibromoethane in the presence of potash at 100-132 C,

Example 1. 6.2 g (0.042 mol of phthalimide and 2.9 g (0.02 mol) of tri-ethylene tetraamine are heated to 195 ° C and kept at this temperature for 1 minute. After cooling to 135 ° C, 21 are added to the mass obtained 8 g or 10 ml (0.116 mol) of dibromoethane and 2.8 g (0.02 mol) of potassium carbonate and heated at the boiling point (132 ° C) for 5 minutes. After cooling to 100 ° C, 50 ml are added to the reaction mixture. water and distilled 40 ml of the distillate. The crystals in the rake of the flask are filtered off, washed with 10 ml of acetone to obtain 3.9 g (45%) K, k-bis- (2

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five

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five

thirty

35

802

-fapapimidoethyl) piperazine, m.p., 242-243 ° C. (Mp. Lit. 240 ° C). The purity of the obtained product was monitored by TLC on the finished plates of Silufol UV-254, eluent - methanol: chloroform 1: 8, with detection in UV light and ninhydrin, Rf 0.43. Calculated N 12.96%. Found N 13.07%. IR spectrum: 1785, 1715 cm -. imide group.

The results of examples 2-14 and their implementation are presented in the table.

Claims (1)

Invention Formula The method of obtaining N, N -bis- (2- -phthalimidoethyl) piperazine formula 1 Oh oh wow by reacting phthalimide with an amino compound, l and h a - y and so that, in order to increase output, simplify the process and shorten its duration, .. As an amino compound, 1, 4,7,10-tetraazadecane is used, the reaction is carried out at a molar ratio of 1,4,7,10-tetraazadecane: phthalimide 1: 1.75-2.1 and 180-195 ° C, formed  the reaction mixture is treated with dibromoethane and potassium carbonate at a molar ratio of dibromoethane: potassium carbonate 5., 8-17.4: 1-3 per 1 mole of the starting 1,4,7,10-tetraazadecane and 100-132 ° С, Note An increase in the amounts of dibromoethane (up to 34.8 mol per 1 mol of triethylene tetraamine) does not lead to a decrease in the yield (yield 40-42%) of the target product, however, this increases the material intensity of the process and labor costs